EP0592654B1 - Device for evaporating preferably liquid substances, in particular reagents, or for preparing or analyzing sampled materials - Google Patents

Abstract

PCT No. PCT/EP93/01037 Sec. 371 Date Dec. 30, 1993 Sec. 102(e) Date Dec. 30, 1993 PCT Filed Apr. 29, 1993 PCT Pub. No. WO93/22650 PCT Pub. Date Nov. 11, 1993.In a device (1) for the evaporation treatment of preferably liquid substances, in particular reagents, or for the preparation or analysis of sample material in a container (6), having a preferably microwave-operated heating appliance (2) and a holder (4) for at least one container (6) in the heating chamber (3), the container (6) being connected to a supply line (11; 11a) and/or to a discharge line (9; 63, 63a), the line (9; 11; 11a; 63; 63a) has in the peripheral region of the container (6) a releasable line connection (43; 45) which is established by the insertion movement on insertion of the container (6) into the holder (4) or severed by the removal movement on removal of the container (6) from the holder (4) as a result of coaxial relative displacement or parallel displacement of the line connection portions (38a, 38b; 23c).

Description

It is particularly common in analytical chemistry to vaporize a substance, especially a reagent such as e.g. a liquid solvent to Separate specified components of the substance.

For this purpose, the substance is heated in a container to accelerate evaporation bring about. The remaining constituents of the substance can then e.g. under Taking into account the weight or weights, draw certain conclusions.

Because of the separating effect that occurs in the evaporation of vaporizable Share of a substance takes place, the evaporation can also be a substance in advantageously separate into certain components or from certain Clean components. The invention thus also relates to the Scope of distillation.

Evaporation and / or processing can take place under vacuum or overpressure Containers take place.

To accelerate the evaporation and / or processing, the is evaporating substance warms up, which usually results in an increase in pressure in the container connected is.

In DE-OS 38 18 697 and in US-A-4 877 624 is a heater for heating and processing Sample material described in at least one container at overpressure, where at the above-mentioned gases increase the pressure in the container A certain pressure is exceeded by a pressure relief valve of the Escape container, get into the closed boiler room and from there by can be suctioned off a suction device. It is also suggested been, the vapors or gases generated by means of a directly to the container withdraw the connected pipeline and evaluate it analytically if necessary.

In the evaporation measures described above, the substance can be in one certain amount in the container or it can be by means of a substance supply line and continuously fed to a steam discharge line and / or removed as steam. In many cases of analytical chemistry it is however, it is common to put the substance in the container in a certain amount, e.g. after weighing, and the steam or gas generated during the treatment to be discharged using a steam discharge line.

In all the cases described above, the container has to be handled more often e.g. fill the fabric or remove treatment residues. One the simpler and quicker handling is the line connection of the Container, however, in particular in cases where the at least one container rotated or heated during heating in the associated device and is pivoted here. as in the previously described, from DE-OS 38 18 697 removable heater is the case. In known configurations must before Removal of the container or after setting it in the heater the existing one Line connection to be opened or closed separately, what handling difficult. In addition, the cable routing is particularly with a rotating holder problematic for the at least one container.

The invention has for its object a device of the aforementioned Art so that it is easy to use and quick deployment or removal of the container in or out of the heater is possible.

This object is solved by the features of claim 1.

The solution according to the invention is particularly suitable for a rotating or and forth, e.g. 360 ° C, swiveling holder for the at least one container. At such a holder requires a rotary connection for the line, so that despite Rotation of the holder a continuous feed and / or discharge through the Management is possible. The holder is preferably set up to hold several containers to record, the line preferably closing in the area of the rotary connection the existing locations for the containers and the number of branches Parking spaces existing line connections are provided.

According to a further development, the line connection to and / or from the container by pushing the container into its standing position in the holder produce automatically and separate automatically by removing the container. It therefore does not need a special screw connection or a special movement to Closing or handling to open the line connection or executed become what would be unfriendly and time consuming and also a would require increased operator attention.

In the embodiment according to the invention, the holder is preferably a guide assigned to the direction of movement of the container, in particular when setting, so that the operator has to pay little attention to whether the

Container in the correct position when inserting or inserting it into the holder located. The guide inevitably guides the container into its predetermined position, whereby the end position of the container is easier in a movement stop Way can be defined.

Within the scope of the invention it is possible that the axis of the line connection is different extends transversely to the approximately horizontal insertion or removal movement or in Longitudinal direction or parallel to the horizontal insertion or removal movement extends. In the first case there is a parallel shift of the intercepts of the Line connection until they are aligned. In the second case, the Line connection according to the invention by a plug connection in the peripheral region of the container be formed with one in the holder and one associated with the container Plug connection part, which interact with each other like a sleeve. In both cases becomes the setting or removal movement of the container for automatic closing or disconnection of the line connection used.

In both of the above cases, the line connection can be sealed easy to implement. In the first case, horizontal, adjacent to each other Mating surfaces between the holder and the container or one between one down facing surface of the holder and an upward facing surface of the container arranged, ring-shaped surrounding the separation point of the line connection Ring seal may be arranged.

In the context of the invention it is further possible that the invention Line connection through a line section extending in the holder and a line section extending in the lid of the container or only through a line section extending in the holder is formed. In the latter case when using a pot-shaped container, the lid of the container through the Be formed holder, the preferably vertical, in the holder side thus formed Cover part extending connecting line section from the cavity of a pot-shaped Container goes out or opens into this.

The invention also relates to advantageous container designs in different versions. As already described, one embodiment consists of that a pot-shaped container open on the top is provided and this container assigned cover part is assigned to the holder or is part of the holder.

Another container design relates to the container from one Form container upper part and a lower container part, for receiving the A sieve or filter base is provided between the container parts, wherein preferably the cavity of the lower container part can be subjected to negative pressure is.

The measure that evaporation takes place in the presence of a vacuum leave is an advantage in all embodiments, because basically the The boiling point of the reagent or solvent drops under vacuum and therefore does not less heating energy, but also at lower temperatures can, whereby the sample material can be spared or heat sensitive Material can be treated at all. This allows both the evaporation fundamentally take place more effectively than in particular take place more effectively, if the vacuum to a Cavity of the lower container part is created, while one in particular with the The reagent or solvent-soaked sample is above it and a sample through the Extraction generated air flow is passed through the sample.

It is possible in the context of the invention, the at least one container to apply negative pressure to the receiving boiler room and vacuum it or aspirate the or each container directly or each container in one to arrange special vacuum tank or room in the boiler room, so that each only the vacuum container surrounding the container at a short distance evacuates are needed, which is possible with less effort and time.

The invention also relates to an advantageous gas purging device for the or the containers for discharging vapors or the like, wherein the reagent or Solvent before inserting the container into the holder in the container can be filled or in the inserted position in the holder by a Feeding device can preferably be fed automatically. In the latter In this case, it is advantageous to use a gas or gas that enables the vapors to be extracted Combine air inlet with the reagent inlet. You can Means may be provided which also allow gas or air to be introduced enable if no reagent should be added, because in many cases only an intermittent supply of the reagent is desired. Both are done preferably through the lid of the container or a part of the lid forming the Holder for the container.

It is advantageous if the vaporous constituents are suctioned off in the container to assign a ventilation valve to the latter or the boiler room through which a gas or Air can be sucked in. This allows a rinsing effect and achieve improved removal of the vaporous components. When using an inert gas as ventilation or purge gas, explosion protection can also be used for reach flammable materials in the container.

The invention is suitable for both automatic and manual introduction of the reagent or solvent in the container, in particular with one automatic feeding this continuously or once, preferably at The container can be loaded.

In all cases, there is a requirement to recognize when the Evaporation process is finished. Solutions for this are also in the form of a Method and associated devices proposed. For one thing proposed to monitor the pressure in the container or in its lines and at a pressure drop over a certain level or a pressure drop that is within a certain time span exceeds a certain pressure drop rate, to reduce or switch off the existing heating. Alternatively or additionally The temperature of the steam in or on the container can also be used for this purpose be measured and if the temperature rises above a certain level or at the temperature rises above a predetermined speed reduced or switched off. The invention also relates to Devices for performing these methods.

Another aspect of the invention relates to the container, parts of the To produce container or additional parts surrounding the container from a material that heats up due to the microwave radiation and thereby the material in the container heated. Such an embodiment is advantageous not only because microwave permeable material can be treated, but also because after reducing or switching off the microwave radiation another one Heating or keeping the material warm is ensured so that otherwise cooling does not result in an increase in steam pressure or a drop in temperature could occur, which could distort the end point determination.

When evaporating preferably liquid substances or when processing or Analyzing sample material is a considerable one of the at least one container Exposed to temperature, which is due to the heating of the sample material and / or Container material through the microwaves and / or possibly a chemical reaction in the container. Temperatures from about 200 ° C to about 500 ° C and arise more. At high temperatures, strength problems arise regarding of the container and / or holder material especially when it is made of resistant Plastic material, such as preferably polytetrafluoroethylene (PTFE-Teflon). The Strength problem is exacerbated by the fact that in a known, from the already DE-OS 38 18 697 removable device against the lid of the container the lower part of the container is prestressed. At a high working temperature, namely when the strength of the container material deteriorates, this leads to preload an additional load on the container, causing deformation or Damage and malfunctions occur. Another, the invention underlying problems therefore consist in the high working temperature and from it following strength problems for the at least one container and / or the holder. The latter problem arises particularly when the holder closes the Container guaranteed, especially when working with overpressure.

Further aspects of the invention for solving the aforementioned problems exist on a temperature therein that acts at least on the container and / or holder and / or to lower the load on the container and / or the holder. A Solution feature for the first problem is the boiler room with air to rinse and thus to cool the container and / or holder outside and / or inside. A Another solution feature is in at least one container on the holder hanging arrangement. This not only applies to the container acting loads significantly reduced, but it also becomes the external cooling surface of the container enlarged because the bottom of the container can also be cooled.

It should be noted that, in particular, with the participation of a reagent the working temperature is highest in the lower area of the tank.

The invention also relates to a cooling device with which the holder and / or the container or parts or parts thereof can be cooled. The danger There is a thermal overload in particular for the container mainly for the lower part of the container, in which the microwaves heat up Sample material is located. The remaining parts of the boiler room Device can be cooled or it could be cooled and only the holder indeed by the cooling air flow that the boiler room from its cooling air inlet traverses.

The embodiment of the invention is particularly suitable for evaporation and Treatment treatments for overpressure. Especially with such Treatment measures result in particularly high temperatures in the container.

However, the invention is also suitable for such treatments of material in the Sample containers which are operated with negative pressure and where the Reaction space is suctioned off in the container and at the same time the reaction space is ventilated is used for the most complete pneumatic flushing of the reaction space. In this case, the container is cooled internally, this then being carried out with an external one Cooling can be combined if the suction air flow from the inside of the container is led to the outside.

The invention also relates to measures that result in a better analysis enable. The analysis result can in many cases be caused by condensation in the Containers especially after the evaporation or Preparation process can be falsified. One aspect of the invention is therefore Prevent or reduce condensation in the tank or take measures that prevent condensate from being used for analysis Sample residue arrives. The formation of condensate can be reduced by the fact that in the upper Area of the container, i.e. on its lid or in its upper edge area Heating is generated, which may be due to the arrangement of materials additional parts can be achieved, which are microwave absorbing and thus in Warm operation by the microwave.

Another measure according to the invention is to have at least one in the container Provide a space for condensate into which the latter flows automatically. Especially when a lower container part without the lid from the holder laterally condensate hanging from the cover is wiped off to the remaining sample material. In a further embodiment of the invention is a Circumferential channel in the container, in particular on an attachment ring, for receiving the condensate provided.

The sub-claims contain features that contribute to problem solving simple and practical and inexpensive to manufacture designs lead, the handling, the assembly or disassembly, the sealing, the Improve heat balance and function and also extend the service life.

Fig. 1

eine erfindungsgemäße Vorrichtung zum Verdampfen von insbesondere flüssigen Stoffen, vorzugsweise Reagenzstoffen oder zum Aufbereiten bzw. Analysieren von Probenmaterial in wenigstens einem wahlweise zu öffnenden und zu schließenden Behälter in vereinfachter perspektivischer Vorderansicht;

Fig. 2

einem vertikalen Teilschnitt eines im Heizbereich der Vorrichtung angeordneten Halters für einen oder mehrere Behälter,

Fig. 3

einen der Figur 2 entsprechenden vertikalen Teilschnitt in abgewandelter Ausgestaltung der Vorrichtung;

Fig. 4 und 5

verschiedene Funktionszustände der Ausgestaltungen nach Fig. 2 oder 3;

Fig. 6

eine erfindungsgemäße Vorrichtung in abgewandelter Ausgestaltung und in perspektivischer Frontansicht;

Fig. 7

einen Behälter der Vorrichtung nach Figur 6 in einer in die Vorrichtung eingestellten Position im vertikalen Schnitt;

Fig. 8

die in Figur 7 mit X gekennzeichnete Einzelheit in vergrößerter Darstellung;

Fig. 9 bis 12

Einzelteile des mehrteiligen Behälters nach Figur 7 ebenfalls im Vertikalschnitt.

Fig. 13 und 14

abgewandelte Ausgestaltungen der Vorrichtung der in der Figur 2 entsprechenden Schnittansichten;

Fig. 15

ein Funktions-Schaubild, aus dem der Temperaturverlauf entnehmbar ist;

Fig. 16

eine Einrichtung zum Messen der Dampftemperatur in schematischer Darstellung;

Fig. 17

ein Funktions-Schaubild, aus dem der Temperaturverlauf entnehmbar ist:

Fig. 18

eine erfindungsgemäße Vorrichtung zum Verdampfen von insbesondere flüssigen Stoffen, vorzugsweise mit Reagenzstoffen oder zum Aufbereiten bzw. Analysieren von Probenmaterial in weiter abgewandelter Ausgestaltung und in perspektivischer Darstellung;

Fig. 19

einen vertikalen Teilschnitt durch einen Halter mit einem daran befestigten Behälter;

Fig. 20

ein Halteelement des Halters in der Unteransicht;

Fig. 21

einen vertikalen Teilschnitt des im Heizbereich der Vorrichtung angeordneten Halters für einen oder mehrere Behälter in weiter abgewandelter Ausgestaltung;

Fig. 22

eine Lösungsmittel- und Gaszuführungseinrichtung gemäß Figur 21 in abgewandelter Ausgestaltung;

Fig. 23

einen vertikalen Teilschnitt des im Heizbereich der Vorrichtung angeordneten Halters für einen oder mehrere Behälter in weiter abgewandelter Ausgestaltung;

Fig. 24

eine erfindungsgemäße Vorrichtung mit einem Halter für Probenbehälter zum Aufschließen und Analysieren von Probenmaterial in perspektivischer Vorderansicht;

Fig. 25

einen radialen vertikalen Teilschnitt durch den Halter im Bereich eines Standplatzes für einen Probenbehälter;

Fig. 26

ein Schutzgehäuse für den Halter bzw. die Probenbehälter in perspektivischer Ansicht.

The invention and further advantages which can be achieved by means of preferred exemplary embodiments and a drawing are explained in more detail below. It shows:

Fig. 1

a device according to the invention for vaporizing in particular liquid substances, preferably reagents or for preparing or analyzing sample material in at least one optionally openable and closable container in a simplified perspective front view;

Fig. 2

a vertical partial section of a holder arranged in the heating area of the device for one or more containers,

Fig. 3

a vertical partial section corresponding to Figure 2 in a modified embodiment of the device;

4 and 5

different functional states of the configurations according to FIG. 2 or 3;

Fig. 6

a device according to the invention in a modified embodiment and in a perspective front view;

Fig. 7

a container of the device of Figure 6 in a position set in the device in vertical section;

Fig. 8

the detail marked X in Figure 7 in an enlarged view;

9 to 12

Individual parts of the multi-part container according to Figure 7 also in vertical section.

13 and 14

modified configurations of the device of the sectional views corresponding to FIG. 2;

Fig. 15

a functional diagram from which the temperature profile can be taken;

Fig. 16

a device for measuring the steam temperature in a schematic representation;

Fig. 17

a functional diagram from which the temperature profile can be seen:

Fig. 18

a device according to the invention for evaporating in particular liquid substances, preferably with reagents or for preparing or analyzing sample material in a further modified embodiment and in a perspective view;

Fig. 19

a vertical partial section through a holder with a container attached to it;

Fig. 20

a holding element of the holder in the bottom view;

Fig. 21

a vertical partial section of the holder arranged in the heating area of the device for one or more containers in a further modified embodiment;

Fig. 22

a solvent and gas supply device according to Figure 21 in a modified embodiment;

Fig. 23

a vertical partial section of the holder arranged in the heating area of the device for one or more containers in a further modified embodiment;

Fig. 24

a device according to the invention with a holder for sample containers for unlocking and analyzing sample material in a perspective front view;

Fig. 25

a radial vertical partial section through the holder in the area of a stand for a sample container;

Fig. 26

a protective housing for the holder or the sample container in a perspective view.

The main parts of the device 1 are preferably effective with a microwave Heater 2 with e.g. lockable boiler room by a door, not shown 3, a holder 4 arranged therein with several, preferably four or six Pitches 5 for containers 6, a suction pump 7, a condensation cooler 8, which in the suction line 9 leading to the suction pump 7 is arranged, several Feed lines 11 or a common and in several feed lines branching feed line for a solvent and an electronic Control device 12, which preferably has a computer and after predefined or enterable programs can work, whereby the Control device 12 a keyboard and a display or a screen for specifying Control data is preferably assigned. In addition, the device 1 is a Assigned scale 10, which is located outside of the boiler room 3, where it is preferably an electronic scale 10, which is operated by an electrical Control line is connected to the control device 12. the latter can be in the Device integrated or in the keyboard and the screen containing Housing be arranged.

The heater 2 is integrated in a cuboid housing 13, from the front accessible and through from the boiler room 3 in the form of a rectangular recess a locking door, not shown for reasons of simplification, can be closed tightly. The suction line 9 and the feed line 11 open through associated openings in the boiler room 3. The holder 4 consists of microwave-permeable material, especially plastic like polypropylene and is a turned part with a lower one Rotating plate 14 and an upper rotating plate 15, between which the container 6 is held are. The rotating part can in the sense of a continuous rotation or a back and forth pivotal movement, preferably be driven by about 360 °. The Rotating plates 14, 15 are connected by a vertically extending connecting part, here Connecting pipe 17, firmly connected to one another so that they connect the connecting pipe 17th protrude radially outward and a common ring recess 18 between them or form individual recesses for receiving the container 6. Preferably on a guide 19 at the top of the lower rotary plate 14 in the area of each parking space 5 provided for the container 6, which is a radially inward Movement control when inserting the container 6 from the side between the Turntables 14,15 specifies. The guide 19 can through a recess 21 with a be flat base 21a formed, the extending in the circumferential direction Width is adapted to the width of the preferably cylindrical container 6.

As FIG. 2 in particular shows, the containers 6 which are identical to one another each consist of a pot part 23 and a flat lid 24, which on the upper edge Intermediate layer of an annular seal 25 rests and the edge of the pot 23 can spread slightly downwards so that it prevents lateral displacement is held. The underside extension 20 with a flat contact surface 20 a for encompasses the rim of the pot 23.

The pot 23 of the container 6 consists of several, in the present case three parts, namely a pot lower part 26, one sealed at its upper edge Pot top 27 and a pot-shaped jacket 28, which extends only to the top of the pot 27 or extend substantially over the entire height of the container 6 can and pots 26.27 picks up with movement. Preferably on arranged lower end of the pot upper part 27, a centering projection 29, which in the The lower part of the pot 26 surrounds, the upper part 27 of the pot having a shoulder 31 on the the upper edge of the lower pot part 26. The bottom 32 of the pot top 27 has one A plurality of through holes 33 or it is perforated in the sense of a sieve. The Pot upper part 27 is also a filter plate 34, preferably a so-called glass or Paper filter assigned, the shape and size is designed so that it is on a Inner shoulder 35 of the pot top 27 can be placed. It is advantageous to provide a step or a slope in the area of the inner shoulder 35, so that in the position of the filter plate 34, a distance between the latter and the bottom 32 is available. In the present embodiment, the individual parts of the container 6 round or cylindrical in horizontal cross section. To the Manageability when inserting and removing the pot parts 26, 27 in and out to facilitate the jacket 28, the latter by a horizontal division 36 in a lower jacket part and an upper jacket part can be divided. The container 6 consists of microwave-permeable material, especially corrosion-resistant plastic, preferably polytetrafluoroethylene (PTFE-Teflon) or tetrafluoropolymer (TFM) or the like. The pot parts 26, 27 or a single pot part can also consist of glass, quartz or ceramic. The individual parts of the container 6 and preferably the jacket 28 can also be made of microwave-permeable material be formed so that they are irradiated by the not shown Heat the microwave generator, which prevents condensation and Reheating is achieved after switching off the microwave. As material for this a plastic is preferably suitable in the material parts, such as particles microwave absorbing material, especially graphite, mixed or alloyed are, and which is known per se under the name Weflon.

The feed lines 11 extend from above to the center of the holder 4 in the heating room 3 and they are by means of connection fittings to a connection plate 37 connected, which is inserted into the connecting pipe 17 so that its peripheral surface abuts the inner peripheral surface of the connecting tube 17. In the connection plate 37 for each feed line 11, an angular channel 38 runs axially first and then radial, which continues as a radial channel section 38a in the connecting tube 17. Of the Channel section 38a can be inserted into an existing one through the connecting pipe 17 Bore fixed sleeve 39 may be formed, the connecting tube 17 to the outside protrudes and thus forms a coupling or connecting pin 41. On the inside The sleeve 39 can also end in a corresponding bore in the connecting plate 37 protrude and thus fix the latter. The sleeve 39 is preferably made of Plastic. This arrangement of the connection plate 37 is provided for a holder 4, that swings back and forth.

In the peripheral surface of the cover 24 there is a plug hole 42, the shape and Size is adapted to the shape and size of the connecting pin 41, so that the Cover 24 with the radial plug hole 42 tightly on the sleeve 39 or Connecting pin 41 can be plugged on. The vertical distance of the sleeve 39 from the Base area 21a is equal to the distance of the plug hole 42 from the bottom of the Container 6. As a result, the horizontal insertion of the container 6 in the associated parking space 5 by the horizontal adjustment movement simultaneously with 43 designated line connection closed and when removing in reverse Direction to be separated. Between the top of the lid 24 and the top Rotating plate 15 is a spring part 44 held on one of these two parts, preferably in the form of a vertically arranged axially elastically compressible sleeve, provided that the cover 24 slightly in the inserted position of the container 6 biased against the pot 23 and thus ensures the sealing of the lid 24. A channel, in particular an angular channel, extends from the plug hole 42 in the cover 24 38b, radially inward, which is preferably in the center on the underside of the cover 24 and thus opens into the cavity of the pot 23.

The suction line 9 is connected to the boiler room 3, so that the Device 1 in the boiler room 3, a negative pressure can be generated. This negative pressure can pass through the existing column or specially provided channels on the one hand between the pot parts 26, 27 and the jacket 28 and on the other hand between the pot parts 26, 27 first into the lower application space 23a and then also continue in the upper application room 23b. Based on these Vacuum effect can be created in the containers 6 during treatment Aspirate steam, due to the passage of the steam and / or solvent through the sample material lying on the filter 34 and / or the sieve plate 32 Treatment is forced.

The suction of the steam can be improved by adding air or a gas in the Boiler room 3 is let in, causing an air or gas flow during suction is achieved. This can be done through a ventilation opening shown in FIG can preferably be achieved with a ventilation valve 40 which is in a channel 40a is arranged in the housing 13, which connects the boiler room 3 with the environment, is preferably accessible from the outside and can optionally be closed and opened and is preferably adjustable. Due to the gas or air flow, the vaporous components from the interior of the Vacuum container 6 and from the boiler room 3 better in the sense of a rinse.

The embodiment according to Figures 3 to 5, in the same or comparable Parts with the same reference numbers differ from the Embodiment according to Figure 2 only in that the lid 24 on the holder 4th arranged or held and thus part of the holder 4. For holding the lid 24 on the holder 4 serves a retaining screw 15a, which is preferably coaxial to the Container 6 arranged vertical hole in the upper rotating plate 15 and in a threaded hole is screwed into the top of the lid 24, the Retaining screw 15a the sleeve-shaped spring part 44 vertically passes through. With the Retaining screw 15a, the head of which is preferably in the top of the upper rotary plate 15 is sunk, the lid 24 can not only be held, but also its Adjust the altitude by screwing the screw in or out. Here is the Lid 24 on its inside by the connector 43 additionally flexible held, which in addition to the flexibility of the sleeve 39 by a radial Movement play of the sleeve 39 can be achieved in the connecting tube 17. At this Design, the connector 43 is intended for a continuous connection. There the lid 24 is held on the holder 4, is used to adjust and remove the Container 6 only the pot 23 inserted horizontally into the parking space 5 or taken. Here, the pot 23 is not only closed or opened automatically, but it will also be an existing instead of the connector 43 Line connection 45 between the feed line 11 and the upper one Application space 23b of the pot 23 produced when inserted and when Take out separately. This line connection 45 is through the channel 38b and the opening 23c of the pot 23 is formed. In contrast to the configuration according to the figure 2, in which the axis of the plug connection 43 runs horizontally, the axis of FIG Line connection 45 vertical.

In the embodiment according to FIG. 3, the lid 24 is also in one High altitude set that the pot 23 with a slight vertical clamping effect can be inserted between the lid 24 and the lower rotating plate 14, the latter can be occupied with a special guide part having the guide 21. There the retaining screw 15a is not limited in the upward direction, can be inserted of the pot 23 of the lid 24 slightly against the spring force of the spring part 44 be pushed up. To facilitate insertion, the bottom of the Cover 24 outside and / or on the top of the cover 24 inside chamfers be arranged.

3, the underside recess 23c in the lid 24 open radially outwards, so that the pot 23 laterally into the recess 23c can be inserted. The radially inner boundary surface forms the Recess 23c one with the upper edge of the pot 23 or the ring seal 25 interacting stop A, the insertion of the pot 23 in the limited desired position. The recess 23c thus also forms here an insertion guide 19.

The device 1 is a device for measuring the in or on the containers 6 assigned existing temperature. These are preferably at least one non-contact temperature meter, in particular an infrared temperature meter 46, which is preferably in the lower region of the plane of rotation of the container 6 is arranged laterally from the holder 4 and to which the container 6 in operation be moved past. The temperature meter 46 is through an electrical control line connected to the control device 12.

An evaporation process is described below with reference to FIGS. 2 to 5. From a material sample 47, e.g. the moisture or fat content can be determined. For this purpose, a quantity of the sample 47 is applied to the filter disk 34 and weighed by means of the scale 10 so that its amount is determined. The one with the sample 47 occupied filter disc 34 is then placed in the top pot 27, the Pot parts 26, 27 may already be in the casing 28 or may be inserted thereafter can be. Then the container 6 with lid 24 (Fig.2) or without a lid 24 (FIG. 3) horizontally into its treatment position on the associated parking space 5 pushed, the line connection 43 or 45 being created automatically. Due to the tension of the spring part 44, the cover 24 is tightly closed, whereby the sample 47 is in the lower region of the pot upper part 27 on the filter disk 34 located (Figure 2 or 3). Then you can start the evaporation process kick off. The heater 2, the holder 4 and the suction pump 7 can be operated simultaneously start, the suction pump having a pressure of 20 millibars and the heater 2, one Can generate temperature of about 80 ° C in the boiler room 3. This treatment time can take about 5 minutes. Here the sample is dried, whereby a existing moisture in the sample is evaporated and suctioned off, which is caused by the in Figure 3 flow arrows 48 is illustrated. The volatile parts pass from the upper application space 23b through the filter disk 34 and the perforated floor 32 in the lower application space 23a and from there through the above-described column or special radial through holes 49 in the jacket 28 or lower jacket part 28a and / or upper jacket part 28b in the boiler room 3, and them are further suctioned through the suction line 9, condensed in the cooler 8 and collected. As a result, the sample 47 is dried. If only drying the treatment of the sample can already be completed be. The amount and the duration of the temperature in the boiler room 3 can by a Timer and / or the temperature meter 46 are determined, the temperature measures on or in container 6. After the treatment stage described above, the Vacuum in the boiler room 3 are reduced, which by opening the valve 40 in the Wall of the boiler room 3 is possible. The valve 40 can be by the Control device 12 automatically open and close optionally.

A next treatment step can be carried out according to FIG. 4 at normal pressure in the boiler room 3 respectively. A certain one is determined by means of a pump or gravity, not shown Amount of solvent 53 (eluent) e.g. about 10 ml, preferably in the center of the upper application space 23b so that the solvent 53 on the sample 47 arrives. At the same time, the heater 2, the suction pump 4 and the holder 4 switched on or driven, with a small amount of solvent, approx. 3-5 ml can be added. The hot solvent 53 passes through the sample 47 and the filter 34, already evaporating, reaches the lower application space 23a, it continues to evaporate (arrows 54) and out of the system as previously described is suctioned off.

In the condensation cooler 8, the solvent vapor can condense and be recovered. There is also a reintroduction by those provided for this purpose Return lines possible (not shown). During this treatment step the passage of the solvent 53 with any steam components that may already be present the filter 34 and the bottom 32 are forced by the negative pressure. This one too Treatment step can be the treatment time by the treatment time and / or Temperature can be determined or controlled.

In the next treatment step according to FIG. 5, one can, if desired Total drying take place. Here, the solvent 53 evaporates completely, whereby the temperature can be maintained by appropriate control of the heater can or the heater can be switched off. This is possible because of the Temperature in the jacket 28 reaches its peak and a post-heating effect and thus the drying effect. Operation of the suction pump can continue until the end of Treatment step are maintained. It can also be caused by the negative pressure Opening of the valve 52 are removed. After this treatment step there is on the filter 34 a residue 47a of the sample material. On the bottom of the The lower part of the pot 26 contains fat (eluate) 47b eluted from the sample material. By weighing the fat and the residue, the desired ones can be obtained Determine test values.

In the condensation cooler 8, which is also exposed to the suction effect of the suction pump 7 the solvent vapor can be condensed and recovered. Means a line, not shown, the condensate to the feed line 11th be returned and reused.

External cooling also takes place in the exemplary embodiments according to FIGS. 1 to 5 of the holder 4 and the container 6 through the gas or through the heating chamber 3 Airflow.

The embodiment of Figures 6 to 8 in the same or comparable Parts with the same reference numbers differ from the above described embodiment by several alternatives. For one, they are Containers 6 are each arranged in their own vacuum chamber 61, which is separated by a surrounding the associated container 6 at a short distance, in particular hollow cylindrical wall or a cup-shaped, preferably also hollow cylindrical housing 62 is formed, the vacuum chamber 61 forming peripheral wall cooperates closely with the lid at its upper edge. Each vacuum chamber 61 is connected to the suction pump 7 through a suction line 63 connected, the suction line 63 - in a similar manner as that Supply line 11 - from the common suction line 63 in a distributor or. Branch piece 64 in the number of existing containers 6 towards them can branch. The common suction line 63 is preferably axially means suitable connection fittings connected to the central manifold 64, the downwardly extending passageway 66 into a below the manifold 65 arranged free space 67 opens, of which the desired number Suction line sections 63a can branch off. This holder 4 is thus for a continuous turning set up. The reagent is added before inserting the or the container is filled in the latter.

As far as the holder of the cover 24 is concerned, this is in accordance with the Embodiment according to Figure 3 by means of the retaining screw 15a and the cable connector 43 held on the holder 4, the pot 23, which here with the Vacuum housing 62 forms a unit from the side between cover 24 and the lower rotary plate 14 can be inserted horizontally and removed again, the lateral guide 19 here through the recess 20 on the underside of the Cover 24 can be formed.

Here too, the line or plug connection 43 is formed by the sleeve 39, which communicates with the free space 67. However, the channel 38b does not open from Center of the container 6 from the bottom of the lid, but it opens into the existing gap between the pot 23 and the vacuum housing 62, the only is dimensioned about 1 or more mm wide. Because the volume of the vacuum chambers 61 is thus small, the negative pressure can be generated with less power become.

If an automatic supply of a reagent or solvent 53 is desired a supply line 11a can be provided, which by means of a suitable Fitting to a feed-through channel which preferably runs from top to bottom 68 can be connected in the lid 24, preferably the Feed-through channel 68 opens into the center of the pot 23. In the 7 an additional flat cover 24a is provided, which on an inner shoulder 23d in the upper edge region of the pot 23, preferably in this is arranged sunk. The arrangement can be made so that the Lid 24a flat on the underside of the lid 24 or the contact surface 20a Recess 20 is present. The additional cover 24a is preferably also made of a material, in particular plastic, that the microwaves such Resistance opposes that it is heated during operation (Weflon). The reagent or. Solvent 53 passes through a vertical central hole 24b in the lower one Cover 24a in the pot 23. It may be the case with the reagent supply lines 11a each separate lines or one from a common line act outgoing line branches, which are connected to a feed pump 60. Because of the one or more feed lines 11a, this holder 4 becomes in operation every now and then rotated here.

In this embodiment too, a ventilation valve 40 is provided, which is in the area the suction pump 7 and can be arranged as a flushing valve in the lid 24, being Ventilation channel 40b and / or 40c with the vacuum chamber 61 and / or the Interior of the pot 23 can be connected, as indicated in Figure 7.

The feed lines 11 a can pass through in the upper rotary plate 15 arranged through holes 15b extend.

Another difference in the design according to FIGS. 6 to 12 is that the pot top 27 with an outer flange 27a on the upper edge of the Vacuum housing 62 rests, which can also have an outer flange. Here, the top part 27 of the pot is on the underside of the flange 27 arranged ring shoulder 27b centered in the vacuum housing 62, the with Edges movement play in it. The is located below the ring shoulder 27b Annular gap between the pot 23 and the vacuum housing 62 the lower pot part 26 is present, the lower end of the upper pot part 27 from below overlaps and can thus be centered. It is advantageous to have one in the lower pot part 26 Place bowl 26a on its bottom, on which there are residues of the sample material collect and then easily removed. The passage between the channel 38b and the vacuum chamber 61 takes place through a vertical channel 27c, which the Flange 27a and the annular shoulder 27b vertically interspersed with the channel 38a flees. If on the underside of the lid 24 or on the top of the flange 27a there is an annular groove connected to the channel 38a, channel 27c need not be in alignment.

In the case of the pot 23 according to FIGS. 7 to 12, the jacket 28 is in the vacuum space 61, with its outer surface on the vacuum housing 62 or can preferably rest with its inner lateral surface on the lower pot part 26. At all In embodiments, the jacket 28 may be a cup-shaped housing, i.e. one have the bottom 28a engaging under the pot 23, which is preferably in the center Hole 28b.

The function of the device 1 of this embodiment is similar to that The embodiment described above, but the boiler room 3 is not directly is evacuated, but only the associated vacuum room 61 by means of the suction pump 7 and the suction line 63, 63a. That is, the free boiler room 3 exempt from the implementation of the extracted vapors. However, there is one Air or gas flow between the vent 40a and the Ventilation channels 40b. This will cause the microwave radiation evaporating constituents of the solvent and possibly the sample material first from the upper application space 23b into the lower application space 23a and then due to existing between the lower pot part 26 and the upper pot part 27 or column in the vacuum chamber 61 and then suctioned further. This one too In the exemplary embodiment, the steam in the cooler 8 can be condensed, recovered and used as Solvents are added again.

In the exemplary embodiment according to FIG. 13, in the same or comparable parts are also provided with the same reference numbers, differs from Embodiment according to FIG. 7 by a different design of the container 6 and another application, namely for cleaning a solvent its evaporation, the impurities on the bottom of the pot 23rd remain. In evaporation mode this is done by heating with microwaves Solvent supplied through the feed line 11a, at the same time the Suction pump switched on and the rotary drive, so that in the one-piece here Pot 23 surrounding vacuum chamber 61 negative pressure is generated, which by radial holes 23d in the upper half or in the upper region of the pot 23 in the latter Interior 23e continues, whereby the solvent vapor is sucked off. Here too the vent valve 40 may improve a desired purging function. To the Increase the residence time of the solvent entering the interior 23e, before it reaches the bottom of the pot 23, there is a downward spiral in the pot 23 Trough 82 arranged into which the liquid solvent from the through hole 76th falls and flows downwards in a spiral. Due to the enlarged path in the Channel 82 results in the desired longer exposure time in which the microwaves can heat and evaporate the solvent.

In the variant of the device 1 according to FIG. 14, in which the same or comparable parts are provided with the same reference numerals and therefore for the purpose Avoiding repetitions not described further is also a one-piece pot 23 provided between the lower rotating plate 14 and the Holder 4 held cover 24 can be pushed horizontally into its working position and again is removable. In this embodiment too, one is provided by the cover 24 Plug connection 43 and the distributor piece 65 extending line 63a are provided at which, however, is not a supply line, but the suction line, which may be connected to the condensation cooler 8 and the suction pump 7.

In this embodiment, the sample material and / or solvent is in the Container 6 entered before the pot 23 is inserted into the holder 4. While of the heating and evaporation operations are evaporable components of the Sample materials and / or the solvent evaporates and the vapors are released after aspirated above through the suction line 9a, the existing in the cover 24 Ventilation valve 40 has an advantageous flushing effect on the interior 23e of the pot 23 causes.

In the embodiment according to FIG. 14, the distributor piece 65 is part of a Rotary connection 83, which with a continuous rotation of the holder 4 a simultaneous Distribution or merging of the channels 38a of the existing container 6 for common suction line 63 allows, the manifold 65 in the pivot hole 84 of a rotary bearing piece 85 inserted into the connecting tube 17 stands still with the holder 4 rotates around the distributor 65. The confluence of the streams takes place in the free space 67 below the distributor piece 65 or its through-channel.

According to FIG. 14, the device 1 is a device for measuring the negative pressure assigned in container 6, through its electrical control line with the control unit 12 is connected and thus a control or regulation of the heater 2 in Dependence on negative pressure enables. In the present embodiment there is a Pressure gauge 86 is provided, which is connected to the tube by a pipe or hose 87 Suction line 63 is connected and thus indicates a negative pressure, which is approximately that Corresponds to negative pressure in the container 6, and which is connected to the control device 12 which is set up by means of an evaluation device, a control signal to be given if the vacuum drops below a specified value. This Design enables an advantageous method for determining the Evaporation end time. If the vaporizable components are evaporated and the evaporation ceases, the one generated by the suction pump 7 falls Suction pressure automatically because the evenly operating suction pump 7 due to Absence of evaporation creates a stronger vacuum. This will End time of evaporation determined and the treatment process through Switching off the device 1 or the suction pump 7, the heater 2 and the Rotary drive for the holder 4 ended, the ventilation valve 40 for Generating a normal pressure can be opened. 15 is the Pressure curve with a pressure drop shown as a curve, the time Z on the The abscissa and the pressure P on the ordinate are shown.

Alternatively, it is possible to determine the end time of the evaporation by To take into account the temperature profile in the container 6. The Control device 12 is set up in the event of a temperature rise above one predetermined level or a temperature rise that is faster than normal takes place to generate a control signal. If the vaporizable components are evaporated in the container and thus the evaporation stops, none Heating energy consumes more for evaporation, which automatically leads to a Temperature increase leads. This determines the end time of the evaporation, and the device generates the aforementioned control signal, whereby the Evaporation process is ended, i.e. the device 1 is described above Way turned off.

The temperature meter 46 can be used to monitor or measure the temperature to be used. It is even more advantageous to set the temperature directly in the Measure suction line. According to FIG. 16, a temperature meter 46a can be used for this purpose serve a resistor or resistance wire 46b, the temperature directly in the Suction line 63 or associated channel sections measures. With increasing temperature the resistance value increases, so that the temperature profile and the temperature can be monitored and measured electrically. The temperature meter 46a is also connected to the control device 12 by an electrical signal line, which at if the temperature is exceeded by a predetermined amount, the above Control signal generated to end the evaporation process. In Figure 17 the Temperature curve with a temperature rise shown as a curve, with on the The temperature T is abscissa and the resistance R is plotted on the ordinate.

In the exemplary embodiments according to FIGS. 7 to 17, external cooling takes place of the holder 4 and the container 6 and also an internal cooling of the container 6 through the gas or air flow.

The configuration according to FIGS. 18 to 20, with the same or comparable parts are provided with the same reference numbers, differs from those described above Refinements in two ways. On the one hand, the containers 6 are in the holder 4 each held in a hanging position by means of a hanging device 91, and for another, an air-flushing device is provided for the boiler room 3, which largely that formed by the suction pump 7, the suction line 9 and the ventilation valve 40 Suction device corresponds, but not for the extraction of vapors but only Cooling air circulation serves.

When holding the container 6 by hanging the holder 4 can be easier and can be produced more cost-effectively, since the lower rotary plate 14 is eliminated can. In such an embodiment, the respective parking space 5 is only on the upper one Rotary plate 15 of the holder 4 is provided, which - apart from that - the design of the Holder 4 can correspond to the previously described configurations.

In this embodiment, containers 6 are used, which are in a downward direction have directed shoulders from their upper edge. In the In the present embodiment, the containers 6 have one at their upper edge horizontal edge flange 92, the lower surface 93 of holding parts of the Suspension device 91 is gripped over and under. The present containers 6 have a neck neck 94 below the edge flange 92, which by a Circumferential bead of the upright container wall is formed and therefore in the area of Neck constriction 94 also constricts the interior of the container. To the Hanging the container 6 can be two on the side and on the bottom on the top Rotating plate 15 arranged angle leg 95 serve the side of the edge flange 92 reach over and under.

In the present embodiment, the angle legs 95 are through the bottom edge a cylindrical sleeve 96 formed in a vertical bore 97 in the upper Turning plate 15 used and by a flange against vertical displacement and is secured against rotation, e.g. positively or by press fit or gluing. How In particular, Figure 20 shows the bottom of the socket 96 by a round Except recess 98, which is open radially outwards and on this side extends into the lower region 98a of the peripheral wall of the bush 96, whereby a lateral, radial insertion opening 99 is formed for the edge flange 92, in the this can be inserted with play, see double arrow. For this is the vertical Distance a between the underside of the rotary plate 15 and the bearing surface of the Angle leg 95 dimensioned somewhat larger than the thickness of the edge flange 92.

The surface 92 b of the edge flange 92 can on the underside of the holder 4 or here the turntable 15 is particularly tight. Preferably in this area a stopper 101 is arranged in the holder 4 and can be clamped against the edge flange 92, whereby the seal is created or improved and the container (6) secured becomes. In the present embodiment, the plug 101 which is circular in cross section is 101 rotatably mounted in a screw ring 102 with little movement, from above can be screwed into the socket 96 and, at its upper end, projects beyond the socket 96 End area attack elements for a manual attack or tool attack for Has screwing or unscrewing. The plug 101 is longer than that Screw ring 102, and it engages under the latter with a flange 101a on its lower End, with its upper end projecting beyond the screw ring 102 by approximately 5 to 10 mm. This outstanding end area is designated by 103. In the plug 101 is a Through channel 104, consisting of a preferably coaxial channel section, the opens at the bottom, and a radial channel section, which in the end region 103 emanates from the plug 101. The radial channel section 104 b is through a Line connection running above the rotating plate 15, e.g. a fixed attachment Hose or tube, with a rotary connection 64 essentially corresponding connected above-described embodiments to which the existing Lead line sections 105 lead and with a common Drain line 63 are connected.

A further through channel 106 is provided in the stopper 101, the part a ventilation device for the container 6. The through channel 106 opens on the underside of the plug 101 in an annular groove 107. At the upper end of the plug 101, a valve screw 108 can be screwed into the stopper, by means of which the To close or open through channel 106 by screwing in or unscrewing and to adjust its size. A corresponding valve 109 can also be used for this purpose be provided in a connected to the through channel 106 from the outside Hose or pipe 106a is arranged. Between the plug 101 and the Valve 109 can branch line 106a in the form of a supply line 11, in particular for the purpose of supplying a reagent, e.g. by means of a pump.

Preferably in the upper opening area of the container 6 is a plug-shaped Guide element 110 arranged, the top of which with the top 92b of the edge flange 92 closes and thus - like the container 6 - with the underside of the stopper 101 seals. The guide element 110 has a cover 110 a coaxially and one of them downward mushroom head-shaped guide head 110 b, which at present embodiment extends approximately into the neck constriction 94 and the The diameter is so large that between it and the inner circumferential wall the container 6 has a small annular gap 5. Between the guide head 110 b and the plate-shaped cover 110 a there is a free annular space 110 c. The lid 110 a lies positively on the divergent wall of the edge region of the container 6 , thereby securing its location. Aligned with the ring groove 107 is in the lid 110 a provided a through channel 106 b, which is independent of the respective Rotary position of the guide element 110 a flow of air or a certain Gas, eg .. inert gas or reagent. Coaxial in the guide element 110 and thus in alignment with the through channel 104 a, there is a second one in the guide element 110, Larger through channel 110 e provided, the part of the discharge line section 105 is.

The function of the embodiment of Figures 18 to 20 can in correspond essentially to the above-described embodiments, so that on a separate description can be omitted. To carry out a Evaporation process or a sample digestion, the container 6, at which are preferably standard containers made of glass or quartz or ceramic is, after entering a sample material 47 horizontally in the Suspension device 91 inserted and by screwing down the screw ring 102 sealed, i.e. closed and at the same time excited. Because of this fixed This configuration is not only suitable for the treatment of fabrics Normal or negative pressure, but also in the case of positive pressure, for which purpose the screw ring 102 is to be closed accordingly. Instead of the screw tension, a in particular elastic tensioning device for pre-tensioning the lid-forming Plug 101 may be provided against the edge of the container.

During the treatment process, the vapors generated can Drain line 63 are sucked off, while the valve 109 (if present) and / or the valve screw 108 is to be opened. Optionally can Reagent can be specifically supplied through the supply line 11. During the Treatment process, the container 6 through the purge air flow 40 b also their underside and thus be cooled over a large area by flushing the Boiler room 3 by means of air sucked through the suction line 9, which at the Feed opening 40, 40 a flows. Here, the steam on the Condense the inside of the tank and run back down as condensate 47 c.

In all of the above-described exemplary embodiments, it is possible and advantageous to use the previously described treatments of a substance in at least one container 6 with the Make reagent or solvent in two or more stages, with the each subsequent stage at least partially a reagent or solvent is used which has been recovered from the previous step treatment and possibly enriched with new reagent or solvent. According to the so-called Nernst distribution the extraction efficiency is greater if it is done in stages than if a single longer extraction is made. In addition, the consumption of Reduced solvent.

The embodiment of Figure 21, in the same or comparable parts with the same reference numerals, differs from those described above Embodiments with a feed device for a reagent or Solvents and a ventilation device for the container 6 in two ways.

On the one hand, the ventilation device designated 40d in FIG Feeder 11b integrated. This enables the Supply line 11a both for supplying the reagent and for aeration or to rinse the associated container 6 so that it is not a separate one Ventilation channel 40b, 40c in the cover 24 is required. According to Figure 21 opens inside of a block 40e a branch line 40f, here a flexible plastic hose, into which Supply line 11a, which starts from the ventilation valve 40 and via a controllable Stop valve 40g and a ventilation gas can supply. The line branch is in Flow direction behind the pump 8, here a peristaltic pump, arranged so that the supply of the ventilation gas is guaranteed even when the pump 8 is not is in operation and no reagent is added. Block 40e is outside the Boiler room 3 arranged or he can - provided he with his attachments microwave-permeable material is - also be arranged in the boiler room 3. The flexible supply line 11a is dimensioned so long that the holder 4 during operation and can execute swiveling movements. It can be for one Container 6 a reservoir 60a, and a feed pump 60 preferably outside of the housing for the boiler room 3, or it can preferably be a common storage container 60a and a common pump 60 may be provided, the supply line 11a in block 40e in supply line branches 11a branches, the number of which corresponds to the number of available containers 6 and the the associated container are connected, wherein they the upper rotary plate 15th and push the cover 24 through (Fig. 22).

In the present exemplary embodiment, the feed line 11a extends in each case lengthwise through the associated retaining screw 15a in the form of a longitudinal channel 15b, which is followed by a coaxial channel 15c in the cover 24, the other Bottom opens out. At its upper end, each retaining screw 15 has one Hose connection, here a connection nipple 15d on which the associated Feed line 11a is attached.

Another design difference relates to the formation of condensate is prevented or that in particular forms in the upper region of the container Condensate is collected and therefore not to that on the bottom of the container 6 located sample residue 47b is able to flow, whereby an analysis of the Sample residue 47b would be falsified.

To prevent condensation, additional heating of the wall is required of the container 6 provided. Wall sections can be used for this, which consist of microwave absorbing material, preferably Weflon, exist, the Container 6 itself can consist of such a material or of such a material Material outside and / or inside can be surrounded. For this, e.g. the container 6 in a cylindrical or pot-shaped jacket 28 can be used, as already shown in FIG 7 is shown. In the case of a container 6 with a lower part 26 and an upper part 27 the jacket 28 extends only to the upper region of the lower part 26 comparable jacket can also be assigned to the upper part 27.

A collecting trough 111 is on the collecting trap Inner circumference of the container 6 is provided. The gutter 111 is located above the bottom of the container 6. It can be formed on the container 6 or on one Insert ring formed, which is inserted into the container 6 and close to the Inner wall rests, whereby it can be attached to it. The gutter 111 can also be arranged above the perforated bottom 32 so that the condensate is not can reach the first sample residue 47a. In one from a lower part 26 and an upper part 27 existing container 6, the collecting trough 111 at the lower end of the upper part 27, being arranged according to FIG. 21 with the sieve bottom 32 or a support for it can be formed in one piece or form a structural unit with it can, the collecting trough 111 and the perforated bottom 32 from the insert ring 112 can be formed or carried on an inner shoulder at the bottom of the Upper part 27 or can rest on the edge of the lower part 26. In the present Embodiment is the gutter 111 by an upper ring projection 112a formed at a radially inward distance from the Inner wall of the container 6 protrudes upward from the insert ring 112. The sieve bottom 32 can rest on another shoulder of the insert ring 112. The gutter 111 is preferably made of a microwave absorbing material, in particular Plastic like Weflon, preferably in one piece with its carrier.

In the exemplary embodiment according to FIG. 23, in the same or comparable parts are also provided with the same reference numerals, the gutter 111 is in one piece arranged on the inner circumference of the container 6. It can be a one or act two-part container 6, according to FIG. 23 is not a perforated bottom 32 for Wearing a filter disc 34 is provided, which has a central upward bearing style 34a can have for manual attack. It is also within the scope of the invention possible that the upper part 27 is not a container upper part in the sense of this word but is only a container attachment ring 114, so that the lower part 26 forms the container 6.

It is advantageous between the container 6 or the lower part 26 and the attachment ring 114 or the upper part 27 to arrange an annular seal to seal to ensure in between. According to FIG. 23, an O-ring 115 is used as a seal provided that between the upper edge of the lower part 26 and the container 6 and a radial shoulder surface 116 of the attachment ring 114 is effective and the Sealing by the vertically directed elastic tension with which the container 6 between the lower and upper rotating plate 14, 15 slightly vertical is compressed, is forced.

If the container 6 laterally after an evaporation or preparation process is pulled out of the holder 4, are on the underside of the lid 24th existing condensate droplets stripped through the top of the container 6, and they flow downwards on the inner wall of the container 6 or attachment ring 114 the gutter 111 without adulterating the material sample 47a or 47b.

Another or additional measure to prevent condensation consists in a material layer or a plate on the underside of the cover 24 To arrange cover 24 or an additional cover 24a 13 assign the microwave-absorbing material to the container 6, see above that condensation is reduced or eliminated due to increased heating.

According to FIG. 23, it is already advantageous for thermal reasons, on the Footprint for the container or containers 6 a plate made of microwave absorbing To provide material.

The microwave absorbing material is preferably a plastic in which microwave-absorbing material is evenly distributed. This can e.g. is carbon or graphite, as is the case in the industry already known plastic material WEFLON is realized. Of the Heat absorbing material portion is too hot after the desired temperature dimensioned. He can e.g. be about 1 to 50%.

Another design difference to the previously described designs 23 consists in that in order to adapt containers of different heights 6 to the Holder 4, a base 117 is provided, the horizontal cross-sectional shape and -size roughly adapted to the horizontal cross-sectional shape and size of the container 6 is so that it fits on the associated parking space 5. It is from Advantage of using the base 117 from a lower base part 117a of a plastic lower heat resistance and an upper base part 117b made of a plastic to form higher heat resistance and a heat insulating property the dimensional stability of the Ensure base. If a bottom plate 118 made of microwave absorbing If material is desired, it is advantageous to place it in the upper base part 117b form-fitting. Such a connector is also recommended between the base parts 117a and 117b to handle the base 117 as a structural unit can. The base plate 118 and the upper base part 117b are perforated.

19 to 23 is indicated and exemplary shown that the inner and / or outer ventilation of the holder 4 and the container 6th does not have to be done from the boiler room 3, but directly from the environment of the Device 1 can take place, namely through a ventilation line, see e.g. 40f in FIG. 21, which is the outside of the boiler room housing and the boiler room 3 extends into the container 6. It is in all embodiments possible, instead of room air an inert gas for cooling in the boiler room 3 and / or to lead to the containers 6, because of explosion protection for flammable Fabrics.

The device according to Figs. 24 to 26 is not covered by claim 1, since e.g. does not contain a line with a rotating connection extending through the cover.

The main parts of the device 201 according to FIGS. 24 to 26 are preferably one with Microwave effective heater 202 with a boiler room 203 through a door 203a can be closed, a holder 204 arranged in the heating chamber 203 with a plurality of preferably four or six spaces 205 for sample containers 206, one each Pressure relief valve 207 for each container 206, which is exceeded when a certain The container internal pressure opens automatically and due to the tension of an elastic Pressure piece closes again and an adjusting device 208 for each valve 207 to adjust its elastic bias, i.e. to adjust the pressure, in which the valve 207 opens automatically, and a cooling device 210 for the Container 206 and / or the holder 204 in the boiler room 203 (Fig. 25).

The containers 206 are configured identically to one another and each consist of one pot-shaped housing 209 with a housing base 211 and a cylindrical, itself vertically extending housing wall 212. The closable by a cover 213 Housing opening is limited by the upper inner edge of the housing wall 212.

The valve 207 is arranged in the upper region of the container 206, whereby preferably its valve member is formed by the cover 213. If exceeded a certain internal pressure in the container 206, the valve 207 opens automatically, so that some of the internal pressure can escape to the outside. This prevents the internal pressure exceeds a predetermined value and the container 206 is overloaded will explode.

The valve seat of valve 207 is on the upper inner edge of the cylindrical housing wall 212 and is formed by a concentric to the cylindrical housing wall 212 arranged cone seat 207a formed, which converges downward. Of the Cone angle is about 45 to about 75 °, preferably about 60 °. A corresponding one Formed cone sealing surface 207b has that in the upper inner edge of the cylindrical Housing wall 212 covers 213 which can be inserted from above.

The holder 204 is a rotating part with a lower rotating plate 214 and an upper one Rotating plate 215 between which the containers 206 are held. The turned part can Meaning of a continuous rotation or a back and forth Pivotal movement, preferably be driven by about 360 °. The rotary plates 214, 215 are through a vertically extending connector, here a Connecting pipe 217, firmly connected to each other so that they the connecting pipe 217th protrude radially outward and between them a common ring recess 218 or form a single recess for receiving the container 206. Preferably on the top of the lower rotary plate 214 in the area of each parking space 205 one Guide 219 is provided for the container 206, which is a radially inward Movement control with movement stop A when inserting the container 6 from the Side between the rotary plates 214, 215 specifies. The guide 219 can by a Indentation 221 can be formed with a flat base surface 221a, whose in Circumferentially extending width to the width of the preferably cylindrical Container 206 is adapted.

As can be seen in particular from FIG. 25, this becomes a parking space 205 associated adjustment device 208 by an adjustable tensioning device 223 educated. 24 and 25, the tensioning device 223 formed by a clamping screw 224, which is accessible from above in a threaded hole the upper rotating plate 215 is screwed. The elastic pressure piece 222 is on the Cover 213 and arranged between the latter and the clamping screw 224. The Pressure piece 222 is preferably formed by a hollow-conical shaped piece, which can be arranged in a top recess of the cover 213. Of the Tensioning screw 224 is an engagement element 225 for a at its upper end Rotary tool arranged. By tightening the clamping screw 224 accordingly valve 207 adjust so that it is at an optional tank internal pressure opens and blows off.

The cup-shaped housing 209 is preferably in a hanging position in the holder 204 held. In the present exemplary embodiment, a sleeve-shaped one serves this purpose Stand 226, here in the form of a cylindrical tube in which the housing 209 of is inserted at the top and with a housing flange arranged at its upper end lies on. With the exception of its upper end, the inside diameter is the Stand 226 dimensioned larger than the outer diameter of the housing 209, so that there is a circumferential gap 5 therebetween. The height of the stand 226 is greater dimensioned as the housing 209 so that the housing bottom in the suspended position is at a distance from the lower rotary plate 214. The lower rotating plate 214 has at each parking space 205 coaxial, in particular a vertical through hole 227 on. Below the inner step surface 228 of the stand 226 are in the latter several circumferentially arranged through holes 29 are provided which preferably run diagonally upwards from the inside out. The purpose of the Through holes 227, 229 will be explained later. Stand 226 can be one have perforated bottom.

The holder 204 is assigned a hollow cylindrical protective housing 231 that is so large is dimensioned so that it is the rotary plates 214, 215 with a small radial distance surrounds, where it rests on the floor 232 of the boiler room 203, and its Height is approximately adapted to the height of the holder 204.

Between the lower rotating plate 214 and the upper rotating plate 215 and the Protective housing 231 is provided with a seal 233, one by rotating or pivoting the holder 204 causes relative movement between the holder 204 and the protective housing 231. In the present embodiment Sealing rings 234a, 234b provided from below or above on the associated Rotating plate 214, 215 are pushed on, abut a shoulder surface 235 and against Longitudinal displacement are secured by a locking pin or split pin 236.

In the present embodiment, the holder 204 is circumferential on three evenly distributed wheels 237 rotatably or pivotally mounted in of the lower rotary plate 214 are rotatably supported and the underside down protrude so that between the bottom 232 and the lower rotating plate 214 Distance 238 is present.

At the lower end of the protective housing 231 is below the lower sealing ring 234a a radial through hole 239 is provided.

The protective housing 231 is by means of a positive-locking pin connection 241 locked against rotation by the holder 204. For this purpose, a Recess 242 can be provided, into which a pin 243 of the underside projects Protective housing 231 encloses a form fit.

The protective housing 231 preferably consists of two half-shells 231a, 231b (Fig. 26) by one or two further pin connections 244 with at least a pin arranged on the half shell and at least one on the another half-shell suitably arranged, the pin receiving recess can be locked together in the fitting position. The protective housing preferably has 231 at its lower end a possibly square flange 245, which at a two-part design is also divided in the axial parting line 246. The Pins of the pin connection 243, 244 can be screwed in by screws be educated.

In the protective housing 231 in the upper area, i.e. however below the top Sealing ring 234 a radial connection hole 247 or a connecting piece arranged by a hose 248 with an outside of the boiler room 203 arranged suction pump 249 is connected. The hose 248 penetrates this Boiler chamber housing 251 in a sealed through hole 251a.

An air inlet 252 is arranged in the boiler room housing 251 and is divided by a plurality small holes can be formed. It is possible to have several spread over the circumference arranged through holes 239 and air inlets 252 to provide.

For a digestion of sample materials filled into the container 206, the Microwave generator (not shown) of the heater 202 and the rotary drive for the holder 204 formed by a rotor turned on. There is a uniform heating of all containers 206 and the sample material contained therein. With this treatment, evaporation occurs mainly in the containers based overpressures and high temperatures. Because usually through the Microwaves only the sample material is to be heated, one chooses as materials for the holder 204, the container 206 and the protective housing 231 microwave-permeable material, preferably plastic, so that the relevant Parts are not heated by the microwaves. For the housing 209 and the Lid 213 also requires a very corrosion-resistant material that is resistant to acids of the sample material that arise during processing are resistant, preferably Polytetrafluoroethylene (PTFE / Teflon) or tetrafluoropolymer (TFM) or also Quartz, ceramic or glass for the housing 209.

It is possible and possibly also advantageous for the housing 209 and / or the cover or a casing surrounding the housing 209 made of a material, in particular To produce plastic that absorbs microwaves slightly and therefore Microwave radiation generates its own heat that supports heating and can also avoid condensation in the container 206.

Such high temperatures occur in the containers during heating which a plastic used, e.g. PTFE, its strength decreased. This The problem could be countered by increasing the wall thickness, but this too larger designs and greater manufacturing costs because the used leads Materials are expensive.

The above-described strength problem of the plastic used does not arise only for the container 206 but also for the protective housing 231 and the holder 204, especially for the upper rotating plate 215, which is due to the bias of the elastic Pressure piece 222 is subjected to a load that it tries to bend upwards. The Using a high temperature resistant plastic for the holder 204 would barely acceptable high manufacturing costs.

This problem is solved by the cooling device 210 according to the invention. Possibly. at the same time as the microwave is switched on, the drive for the suction pump is activated 249 turned on, which generates a cooling air flow 253, which is at the air inlet 252 enters the boiler room 203, across the boiler room 203 to the or radial through holes 229, the distance 238, the through holes 227, the Circumferential gap S, the radial through holes 229 and between the holder 204 and the protective housing 231 existing ring clearance 254 to the hose 248 and Suction pump 249 extends from which is blown to the outside. Of the Air flow path is illustrated in Fig. 2 by arrows. The cooling flow 253 for the other container 206 runs accordingly. Through this air flow the Housing 209 cooled in its lower area over the entire surface, the air flow absorbed heat is dissipated. It is advantageous for the housing base 211 to form hemispherical. This results in a trouble-free advantageous Distribution of the air flow towards the circumferential gap S.

It may be advantageous to postpone the cooling device 210 after a certain time Switch off the microwave generator. With the above The cooling device 210 according to the invention thus simultaneously cools the Holder 204 with its individual parts, the protective housing 231 and the container 206, the latter being external cooling.

The above-mentioned problem of strength of the plastic at operating temperature applies also for the cover 213. This is why a stabilizer is assigned to it, here in the form an upper cover plate 213a, which between the lower cover plate 213b and the elastic pressure piece 222 is arranged. The upper cover plate 213a is made made of a plastic of higher strength than the strength of the lower cover plate 213b. The upper cover plate 213a is preferably in a recess in the lower one Cover plate 213b inserted.

Claims (6)

1. Device for the evaporation of in particular liquid substances, preferably reagents, or for the preparation or analysis of sample material, having at least one container (6)

   which comprises a pot (23) and a lid (24), having

   a heating appliance (2) effective by means of microwaves,

   a holder (4) in the heating chamber (3) of the heating appliance (2) for at least one container (6),

   the container (6) being connected to a line (63),

   which line extends through the lid (24) and the heating chamber (3) to the outside, out of the heating chamber,

   the container (4) being mounted rotatably around a vertical axis and being rotatable by means of a drive,

   and there being provided in the line (63) a rotatable connection having a vertical axis of rotation,

   which rotatable connection, upon rotation of the container (4), ensures a continuous supply and/or discharge through the line (63).
2. Device according to claim 1,
   characterised in that,

   the rotatable connection is arranged centrally.
3. Device according to claim 2,
   characterized in that,

   the line (63) is connected with a connector piece (64) which is rotatably mounted in a rotation-bearing hole (84) of the holder (4), and in that the line (63) extends through the holder (4) to the container (6).
4. Device according to any preceding claim,
   characterised in that,

   the line (63) has in the peripheral region of the container (6) a releasable line connection (43; 45) which is established by the insertion movement on insertion of the container (6) into the holder (4) or severed by the removal movement on removal of the container (6) from the holder (4) as a result of coaxial relative displacement or parallel displacement of the line connection portions (38a, 38b; 23c).
5. Device according to claim 3 or 4,
   characterized in that,

   the holder (4) has a plurality of positioning places for containers (6) distributed around its axis of rotation and there branch off from the line (63), in the region of the rotatable connection, line branches (63a) which extend to the containers (6).
6. Device according to claim 5,
   characterised in that,

   the line branches radially penetrate the lid (24) with angled line branch sections (38a, 38b) and emerge at the underside of the lid (24).

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